Andrew S Forman

US Patent:

55853838, Dec 17, 1996

Filed:

May 3, 1995

Appl. No.:

8/434082

Inventors:

Andrew L. Forman - Scotch Plains NJ
Sean R. Holihan - Dayton NJ
Guy R. Humphrey - Belle Mead NJ
David M. Lashen - Edison NJ
James A. McCauley - Belle Mead NJ
Paul F. McKenzie - Yardley PA
Ross A. Miller - Fanwood NJ
Pascal H. Toma - Piscataway NJ

Assignee:

Merck & Co., Inc. - Rahway NJ

International Classification:

C07S 7300
A61K 3158

US Classification:

514284

Abstract:

By this invention, there is provided a process for producing crystalline 4,7. beta. -dimethyl-4-aza-5. alpha. -cholestan-3-one of structural formula (I) from 4,7. beta. -dimethyl-4-aza-5. alpha. -cholestan-3-one oil. ##STR1## This crystallization process of the present invention comprises crystallization of the oil optionally containing residual solvent with vigorous but controlled agitation. Preferably, this crystallization process is carried out at select and controlled temperatures. Further, 4,7. beta. -dimethyl-4-aza-5. alpha. -cholestan-3-one has been found to exist in at least two novel polymorphic nonsolvated forms, herein referred to as Form I and Form II. Form I can be prepared pure by careful control of the crystallization process.

US Patent:

54498198, Sep 12, 1995

Filed:

Jun 6, 1994

Appl. No.:

8/254805

Inventors:

Andrew L. Forman - Rahway NJ
Ralph J. Magliette - Piscataway NJ
Donald McKinney - Freehold NJ

Assignee:

Merck & Co., Inc. - Rahway NJ

International Classification:

C07F 938

US Classification:

562 13

Abstract:

Disclosed is a process for removing by-product phosphorus-containing (PO. sub. x) materials, alendronate and alendronate byproducts from crude mother liquors in an omega amino-1-hydroxy-C. sub. 2 -C. sub. 6 alkylidene-1,1-bisphosphonic acid synthesis process, e. g. alendronate sodium. Calcium chloride is added first to the crude mother liquors, then calcium oxide to precipitate the PO. sub. x materials, then neutralized to about pH 7 to complete precipitation. Substantially all of the alendronate sodium active ingredient is removed from the precipitate. Following filtration, the PO. sub. x filtercake can then be disposed of by incineration, landfilling or reclamation of usable phosphorus as fertilizer. The remaining filtrate can then be further treated in an environmentally acceptable manner by wastewater treatment or recycling to the process.

US Patent:

55896910, Dec 31, 1996

Filed:

Jun 6, 1994

Appl. No.:

8/254213

Inventors:

Andrew L. Forman - Scotch Plains NJ
Ralph J. Magliette - Piscataway NJ
William A. Vaughn - Avenel NJ
Richard R. Dauer - Longmont CO

Assignee:

Merck & Co., Inc. - Rahway NJ

International Classification:

C09K 300

US Classification:

25218211

Abstract:

Disclosed is a process for recovering and recycling waste methanesulfonic acid (MSA) and phosphorous acid (H. sub. 3 PO. sub. 3) in a bisphosphonation process for reuse in the process. The recovery process involves treating a waste crude mother liquor stream with HCl to remove sodium ion, as sodium chloride, recovering HCl--H. sub. 2 O by atmospheric distillation, separating and dehydrating a mixture of methanesulfonic acid and phosphorous acid by vacuum distillation for recycle. The substantially dry methanesulfonic acid and phosphorous acid, and previous HCl, can all be recycled back to the process for reuse.